Ma Qualitative Inorganic Analysis

Wet Tests for Basic Radicals
Following Extracts of the sample are to be prepared:
❑ Water Extract of sample for detection of Na+ & K+:

Evaporate the clear extract to dryness and perform flame test with the dried mass.
• If golden yellow flame, Na+ present and confirmed
• If pale violet flame by naked eye and crimson red through double-blue glass, K+ present and
confirmed.
❑ HCl extract for detection of Pb++, Fe3+, Co++, Ni++

❑ Conc. HNO3 extract for detection of Mn++, Cu++
❑ Dilute acetic acid extract for detection of Ba++, Sr++, Ca++
❑ NAOH extract for detection of Pb++, Zn++, Al3+
Analysis of Insoluble Part

List of insoluble compounds:
Coloured: Ignited Cr2O3 (deep green), Ignited Fe2O3 (rusty brown),
White: BaSO4, SrSO4, PbSO4, CaF2 (also grey), Al 2O3, SnO2
Isolation of Insoluble Part:

After conc. HCl extract of the sample, wash the residue several
times by hot water containing a little dil. HNO 3 and finally dry it.
WET TESTS FOR BASIC RADICALS
Experiment Observation Inference
Conc. HCl Extract: Heat with conc. HCl. If white Golden yellow Pb++ conf.
crystalline ppt deposits on cooling, Pb ++ is indicated. crystalline ppt
Separate ppt and solution (HCl extract). Dissolve the
residue in a little water and add KI solution.
Use the HCl extract for following tests: 1. Blood red colour 1. Fe3+ conf.
1. Solution + NH4SCN Solution
2. Solution +Conc. HCl + NH4SCN. If any red color 2. Deep blue colour 2. Co++conf.
discharge with SnCl 2 + acetone
3. Solution + a slight excess of ammonia. Ppt if any, 3. Rosy red ppt. 3. Ni++conf.
filter. Add DMG reagent to the filtrate.
Conc. HNO3 extract: (Perform while testing for PO43-)

4. HNO3 Extract + sodium bismuthate(a pinch). Shake 4. purple color. 4. Mn++conf.
and settle
5. HNO3 Extract + excess ammonia to distinct smell. 5. Chocolate brown 5. Cu++conf.

Discard the ppt if any. If the solution is deep blue, Cu ++ ppt
is indicated. Acidify with acetic acid and add
K4[Fe(CN)6] reagent.
Dil. acetic acid extract (For Ba++, Sr++ and Ca++)
Heat the sample with dil. acetic acid and with the solution test for Ba ++, Sr++ & Ca++
as in group IV.
To a few drops of solution, add K2CrO4. If yellow ppt, Ba++ present and confirmed.
*In that case add the reagent to the rest of the solution to precipitate out Ba ++ and filter.
(*If Ba++ absent, proceed to the next stage with the rest of the solution)
Ppt: Yellow. Solution: Add solid (NH4)2SO4 and dissolve. If white ppt., Sr++
Ba++ confirmed. present and confirmed*. Filter.
(Flame test may
further be performed) Filtrate: Add saturated (NH4)2C2O4 followed by NH3 drop-wise
and scratch the walls of test tube with glass rod. A white ppt.
confirms* Ca++.
*flame test may be done with the ppt in both cases.
NaOH Extract: (For Pb++, Zn++ and Al+++)
*If S= is present, heat the sample with a few drops dil. HCl to remove H2S completely. Add excess
of fresh dil NaOH , heat carefully and filter, if necessary.
(* if S= is absent, treat directly with NaOH ). To the extract pass H2S. If ppt, filter.
Residue Filtrate
If white ppt, Zn++ is present and Filtrate: Acidify with dil. HCl. If any ppt ,
confirmed. filter and boil off H2S completely from the
If black, Pb++ may be present and Zn++ filtrate and divide into two parts.
may be present along with. (i) To one part add excess of NH4OH till
Dissolve the ppt by heating with dil. strong smell of NH3. White gelatinous ppt
HNO3 and neutralise the solution with confirms Al3+
excess NH4OH. If any gelatinous ppt Pb ++
may be present. Filter. (ii) To the other part add excess of fresh aq.
PPt.: Dissolve the ppt in dil acetic acid NaOH. To a few drops of the alkaline
and add K2CrO4 reagent to the solution. solution, add drops of Alizarin-S reagent
A yellow ppt confirms Pb++ followed by dil. acetic acid drop wise to just
discharge the violet color of the reagent. A
Filtrate or solution: Pass H2S. If white red coloration or ppt. compared to a blank
ppt, Zn++ is confirmed. confirms Al3+
Analysis of Insoluble Part
Colour of insoluble part &Test Observation Inference
White :
Flame Test Apple green flame BaSO4
Persistent crimson red SrSO4, CaF2
Transient brick red CaSO4
Livid blue PbSO4,
Test for F-: Heat with conc Oily liquid and the issuing vapour CaF2
H2SO4 solidifies water drop
Blue fluorescence SnO2

Fluorescence Test
Green/Rusty red Green bead Cr2O3

Borax bead test Yellow bead Fe2O3
Green Yellow mass Cr2O3

Fusion Test for Cr- compound
-
Insoluble Part
Al2O3:
Fuse the insoluble part with KHSO 4 in a fusion tube for few minutes, cool and extract
by heating with dil. HCl. Add excess of fresh NaOH to make it alkaline. With the
solution perform following tests :
Divide into two parts
1.To first part add solid NH4Cl, heat to dissolve. A white gelatinous ppt confirms Al 2O3
2. To the second part on a spot plate, add Alizarin-S reagent followed by dil. acetic acid
drop wise to just discharge the violet color of the reagent. Red color or ppt
compared to a blank confirms Al 3+.
PbSO4:
Heat the insoluble part with strong ammonium acetate solution, centrifuge and divide
the centrifugate into two parts:
To one part add K2CrO4. A yellow ppt confirms Pb ++.
Acidify the other part with dil. HNO 3 and add Ba(NO3)2 . A white ppt confirms SO4=

Ma Qualitative Inorganic Analysis

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Wet Tests for Basic Radicals

Following Extracts of the sample are to be prepared:

❑ Water Extract of sample for detection of Na+ & K+:

❑ HCl extract for detection of Pb++, Fe3+, Co++, Ni++

Analysis of Insoluble Part

White: BaSO4, SrSO4, PbSO4, CaF2 (also grey), Al 2O3, SnO2

Isolation of Insoluble Part:

Conc. HNO3 extract: (Perform while testing for PO43-)

5. HNO3 Extract + excess ammonia to distinct smell. 5. Chocolate brown 5. Cu++conf.

Colour of insoluble part &Test Observation Inference

Blue fluorescence SnO2

Green/Rusty red Green bead Cr2O3

Green Yellow mass Cr2O3

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